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Au NR synthesis step 4: Coating procedure for organic solvent soluble Au NR
The strategy we employ to prepare organic solvent is to coat the Au NR
with a molecule containing a S-H (thiol) group to covalently bind the
coating to the surface of the Au NR. Commercially available coatings include
thio-polystyrenes, thio-alkanes, and thio-lecithin derivatives. We have also
prepared a series of thio-mesogen derivatives at the facility. The
solubility of the Au NR in solution depends on nature of the coating, with
longer polymeric coating tending to give better solubility in solution.
Chemical |
CAS # |
Thio-alkane
(10C)
|
|
DPPTE (Avanti polar lipids) |
|
Thio-polystyrene
(polymer source) |
|
THF |
|
Toluene |
[65-45-3] |
Other solvents such as
chloroform or DMA may be used |
|
Materials List
balance |
weighing boat / paper |
pipete |
magnetic stir plate / bar |
glass vial (20mL) |
Au NR solution (CTAB coated) |
inert gas supply (nitrogen or
argon) |
rubber septum |
|
|
|
|
|
|
|
Thiol (SH) are susceptible to self oxidation converting 2 S-H bonds to a S-S
bond, resulting in weaker bonding to the Au NR surface. To prevent this problem, the coating reaction may be run under and
inert gas such as nitrogen or argon, described below. That being said,these reaction may be run successfully without using
an inert gas if unavailable.
Step 1: Selection of coating material
- The choice of coating material depends on the application for the
material. For Au NR soluble in organic solvent, longer chain polymers
are simple to prepare. In this case, the polymer chains act as 'brushes'
that prevent the rods from aggregating. Shorting coating can be better
for incorporation into polymer networks to avoid micro phase separation,
while the phosphatidyl choline is best for biological applications. Coating is an exchange
process, with CTAB replaced with the coating material. Both CTAB and the
thio-coatings described here are soluble in the solvent tetrahydrofuran,(THF)
Step 2: Coating
- One question for preparing the coated Au NR is how much coating material is needed to coat the rods
From our experiments, we estimate that 10 to 15% of the initial gold is actually converted
to Au NR. This corresponds to approximately 1.45E19 gold atoms in the
solution of Au NR. If we grossly overestimate the number of Au atoms on the
surface of the Au NR as half of this number, this corresponds to ~7.25E18
surface Au atoms, or ~1.25E-5 mol of surface Au atoms. Therefore, for a
coating with a molecular weight around 500 g/mol, 6mg of coating would be
required to coat the rods. In actuality, this number could be much lower.
- We have achieved best success when equi-volumes of Au NR solution /
THF are used. Use a graduated cylinder to measure the Au NR volume if unknown.
- Measure out an equal volume of THF to the volume of Au NR solution in a glass vial
- Weigh out the appropriate amount of thio-coating material. Based on amounts in this procedure,
thio-polystyrene (20 mg); thio-alkanes (3 to 4 uL), DPPTE (4mg)thioethanolpho
- Dissolve the thio-material in the THF
- Strongly stir the aqueous Au NR solution and add the THF/thio-coating solution dropwise,
approximately 1 drop per minute. After all the solution is added, allow to stir for another
30 minutes if coating with polystyrene. If using a non-polymer coating, spin for at least 4 hours before
proceeding to the next step.
- Stop stirring the reaction. At this stage, the Au NR may have precipitated out of solution. This is
expected. If the Au NR have not precipitated, centrifuge the solution for about 20 to 30 minutes at high speed.
- Carefully remove the solvent from the rods using pipette.
- Residual water on the Au NR will result in the formation of an emulsion when the organic
solvent is added to the solution. Gently flow air over vial to remove the water, or place in a 40oC
oven overnight. Temperatures over 60oC may change the shape of the rods
- After the rods are dry, add 2 to 5 mL of an an organic solvent such as toluene or chloroform to
the vial containing the Au NR. To suspend the rods in solution, gently shake the vial. If the
rods are still stuck to the bottom, a vortexer or sonication bath to resuspend the rods in solution
The preparation is now complete.
- Over time, the rods may fall out of solution. When this occurs, sonicate the solution to resuspend
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